Manufacture of nitrogen



March 3-1.

' F. A. RUDOLF MANUFACTURE OF NITROGEN HHIIH Filed Oct. 15. 1920 firizhmmf/Hiudmf BY ATTORNEY Patented Mar. 31, 1925.

UNITED STATES PATENT ore-ice.

rn'anmaim A. RUDOLF, or JAMAICA, new YORK, assrenon ro' GERALD M. LIV- ruesrorz, rnus'rnn.

mancracrnnu or uzraoenu.

Application filed October 15, 1920. Serial n 417,254,.

ments in the Manufacture of Nitrogen, of

which the following is a specification, reference being had therein to the accompanying drawing.

My invention relates to improvements in the recovery of nitrogen from. a mixture which may be rich in nitrogen and con-' taining carbon monoxide,'carbon dioxide, small amounts of hydrocarbon, andpractically no oxygen evolved from certain types of gas producers and hydrocarbon generators. This mixture of gases may analyze 60% or more of nitrogen, the major portion of the rest of the mixture being carbon monoxide with varying percentages of the other gases mentioned. Oxygen as a free gas is entirely absent, or present in only small quantities. The invention is applicable to processes where comparatively pure nitrogen is required and where the carbon monoxide content of the gas is not suiiiciently high to render the gas valuable as a fuel.- I

In the accompanying drawings, I have illustrated a suitable form "of apparatus such as may be employed in: the practice of the invention, the samebeing. illustrated longitudinal section, parts being broken way. I

' Referring to"said drawing, 1 indicates "the reaction chamber which may be of cast iron suitably supported and which is filled with the reacting oxide preferably in granular form. i'z llhis chamber preferably comprises threesections numbered respeetiyely .2, 3 and ancl the oxide in the chamber indicated by the reference character Qwlien once reduced is not again regenerated but is used-- in-the'reduce'd form as a precaution against acc dental introduction of oxygen.

to carbon dioxide'takes place. The final section 4; is intended as a precaution for the final cleanup of carbon monoxide. There are no partitions of anylrlnd between theseseveral sections. 5 is thecombustion chamberand 6 a boiler, heat economizer, heat exchange or reaction chamber for with a regulate indicates the actual reaction chamber wherein the oxidation of carbon monoxidemaintaining the heats of reaction in any step of any process and these; tubes may be located either above or below :the reaction chamber 1. The fuel for the combustion chamber 5 is in,the form of a; gas mixture (CO-N) and air, the formerientering by way of the pipe 7 controlled by the valve 8, and the air by the pipe 9 controlled by the valve 10. The gases from the combustion chamber 5- passes upwardly "aroundthe reaction chamber -1, between the tubes 6 and out by way of the pi e.- ll controlled by the damper 12, or provi ing'the damper Y 13 is open these gases maypjass to the atmosphereby way of the pi pe l l. From I the reaction chamber 1 the gases may escape to a 'gas washer and g'asomete'r (not shown) subject to the control of the valve 15 upon pipe 16, or the regenerative gases may escape tothe atmosphere through the pipe 17 controlled by the valve 18; Air may also be admitted to the neaction chamher, 1 by way of the valve 20. y

The mixture oi -carbon monoxide and nitrogen is obtained from any suitable source such as a-gas'producer or hydr0carbon generator wherein a mixture of carbon monoxide and nitrogen is produced and the hydrocarbons have been condensed. out.

-For thepurposdof illustration I will assume a gas mixture containing about nitrogen and 35% carbon monoxide. This gas enters throu hthe,pipe 7 and is mixed amount of air from the pipe 9, the mixture being ignited. at the burner 21 in the chamber 5, the mixture being so regulated that the products of combustion will contain some carbon monoxide (not over 10% and preferably not under 5% as a matter of insurance.) For urposes of insurance againstunnecessary ntroduction of oxygen into the combustion chamber thro'ugh the walls, etc., the pressure in the chamber is maintained slightly above that of the surrounding atmosphere by means of suitable fans and exhausters not shown.

the pipe 19contr0lled by I The reaction chamber being fully charged opemiimz or during rewznemtisn 0% L133 oxide ihese gases may 33% e ,a'usi ed through the; outlet 17 0 the afimoaplzere, hut during ifg'il operatisxz Hwy fllmugh the pip .16 to a Sui/ skis "washer am} y 0123215213 the waive 8 being 015 coursa clused.

Af'aey the metzeiiic ezids in the Yeast-i021 01 reams-(L no atiempt 1s it and 1%; preferably in order to ghfl get into in handiing. 2f the :foilowcu v Jim 95 m6 ms,

'g m-ted may other ia a; met-:12 may be The. 135%; 'i'fifi-flrl sac-Minn 4% if; s0 cumrofied. ihat very ham mid}; enters; int; 2' 50B. 5 its purpoare is insumnca 321L313 01f cm'beisa' mozmxiiia 1&0, gasomeima Afer reewim:

50 that the main p0 r: V ides in :ssconfl sc cticn have been reduced which 1215.3 be: 'gcvr\. ua-- tenm'ined 5 31 i1 smiiiabka metfwd, if

bustier sfwtha stopped in ma bustion Laban 5 Valves 8., 1&3,

damage. the g! the aducad; me sectien am 1 Sui awed alumna by mmng in multiple ms {uni one I :lfiernaia The gasm 1 Haida-:2. ii H1 smafi pemenmgaa ream: Th5 mine:

. m uxidize gases 115213 2e amted from the niw tmgem by qlisab'e well knewn means either chemi fifififi qiphysical, preferably the latter whichfhja'y be donev by liquefication 1:0 the. propertinpemt-ure ami pressure m remove these gisisfis to the" extent. dfisirefi any well 3:110:52; form of-appamtlis being employed. for the puxrpuse, 1 claim: 3,. The method of mecbvering nitrogen from mixtures containing}? ami CG 'wilih cem'pzises burning mice 6f :1 limited supply of air to e-fieci; incmnpleiie cfimbus'hien 'nnly, passing the gases of comimstian Enough refra'qtnry mat'sxiai wry material is reduced regemratiiig wa- 100N101; 01: said retfmctary' x'm-teriai 0113513; While keapipg ishfi remainder in a reduc'es cuiuiitiml, and thereafter maintaining th lmfii er in its raduced conditicn. '45." methmi of lfiG-OYGIiI-lf; nifirogen from miximea cimtaining' the same' which cmnprifies burning said n'lixtur'es in the presauca 111% a incompie-ie mmbustion only, passing. the 559.54% 01 cumbustien through a heatare 1 ngai', the haatedgases through unwary znszterial'to oxidize saiii gases *6 msje x refmstery material is reduced, 2?; portion of said, refractory nmtmiiai whila keeping the mmainder' mud. e 36. am difiimgandthereafter main Eu tar in its reducmicmdition.

521ml of rewvering nitmgen me cmltaining 11m iii-l,

. 1mg mixture in. the, pr-as united suppiy 01?? air to fifiect i2 mbusfiiion gmiy, paasingtba gasses thrnugh' a heat ezzchangaig mailed gases. that: b a badgy of; :33; nmiariai of subsmmiml length, 9 gases Mun-eh sai i refmcim'y refrszetary Ira-maria snbstzmtiaiiy :1? tbs hey wiul a, mmnm'inmg the 16 in its 3 gartzon at. we, efi'tmnce of i? "a'ad usefl cmzdrtipn, and mzmlmining the last i'aaucigd conchtmn mmlizimnsal ,QUI'MCK 1'21 its ih'mughsut the r 232, the iaiimfi 311a: zmpa. wins 1 m ape-whom 4;. The gum-had v01? qwavvririg niirogfin fl'nm mixtures cnnminiz'ag {3G and 'N which comprises inmzing said mixture inthe yaw-s mmtfluf s. 'Eimited a ugtryiy .9. air in efl'eat i1" 0mm) wmbustion 021 I gnawing; the gases at cnmbusiisn thrmigh a, 11s?" exchanger, passing the heated. t w :1. bad 0f irefi'aeim-y ma t arizzi 11G azldim antisa 4301. l sting fin, 0pm; 21 5011 that the (mid- 1km of he gases am? siu'mlwnamis: re-

duziion m the. gases is siibstantially can 12% 5111.226, distance 15mm the'end 0f the limited supply of air to effect said gasefi, 1

said mixture in the pressaid gases,flwhereby said body While maintaining the portion at the entrance ofthe gases in its reduced condition, and maintaining the last mentioned portion in its reduced condition throughout the rest of the time the apparatus is in operation;

5. In a process of the character described, the steps ofreducing a refractory body throughout substantially its length by the passage therethrough of the gases to be treated, regenerating a portion ofthe reduced material, and maintaining the remainder in its reduced condition during the remainder of the passage of gases therethrough.

6. In an apparatus for recovering from gaseous mixtures a combustion chamber, means for introducing regulated quantities of the mixture and air to the combustion chamber, means for burning the mixture in said chamber, a heat exchanger in said. combustion chamber, a tube of refractory oxidizing material in said combustion chamber extending transversely therethrough, means forintroducing the gases of combustion into said tube, means in said tube for disposing of excess oxygen which may enter, means for passing off the mixture when treatment is complete, and means for regenerating a portion of said refractory material which has been reduced by passage therethrough of the gases.

7. In an apparatus for recovering Nfrom gaseous mixtures a combustion chamber,

- means for introducing regulated quantities reduced.

of the mixture and air to the combustion chamber, means for burning the mixture in said chamber a heat exchanger in said combustion chamber,.a tube of refractory oxidiz- Zing material in said combustion-chamber extending transversely therethrough, means for introducing the gases of combustion into said tube, means in said tube for disposing of excess oxygen which may enter, means for freeing the gases of all traces of carbon monoxide, and means for regenerating a portion of said refractory material which has been reduced by passage therethrough of the gases.

8. An apparatus for use in the separation of nitrogen from a mixture of nitrogen and carbon monoxide, comprising a combustion chamber for burning themixture, means for introducing regulated quantities of the mixture and air to the combustion chamber, a tubular chamber extending transversely through the combustion chamber, through which tubular chamber the gaseous products of combustion are conducted from, the combustion chamber, finely divided metal in the first portion of the length of the tubular chamber and a metallic oxide in the remaining portion of the tubular chamber, and means for supplying air to the second portion of saidjtubular chamber to reoiridize the metallic oxide when it has become In testimony whereof I hereunto-aifix my signature.

FERDINAND A. RUDOLFQ 

